CN114184706B - Method for measuring content of homotrichlorotrinitrobenzene by gas chromatography - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 16
- 239000000523 sample Substances 0.000 claims abstract description 45
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000012488 sample solution Substances 0.000 claims abstract description 14
- 238000010606 normalization Methods 0.000 claims abstract description 6
- 239000012085 test solution Substances 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 3
- LZMONXBJUOXABQ-UHFFFAOYSA-N 1,3,5-trichloro-2,4,6-trinitrobenzene Chemical compound [O-][N+](=O)C1=C(Cl)C([N+]([O-])=O)=C(Cl)C([N+]([O-])=O)=C1Cl LZMONXBJUOXABQ-UHFFFAOYSA-N 0.000 abstract description 17
- 238000004458 analytical method Methods 0.000 abstract description 7
- WUMOEIUPWHYXBM-UHFFFAOYSA-N 2,3,4-trichloro-1,5-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC([N+]([O-])=O)=C(Cl)C(Cl)=C1Cl WUMOEIUPWHYXBM-UHFFFAOYSA-N 0.000 abstract description 6
- VYZAHLCBVHPDDF-UHFFFAOYSA-N Dinitrochlorobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 VYZAHLCBVHPDDF-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007812 deficiency Effects 0.000 abstract description 3
- UATJOMSPNYCXIX-UHFFFAOYSA-N Trinitrobenzene Chemical compound [O-][N+](=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1 UATJOMSPNYCXIX-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000002360 explosive Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- YXODCXKIYJZGJP-UHFFFAOYSA-N 1,2,3,5-tetrachloro-4,6-dinitrobenzene Chemical compound [O-][N+](=O)C1=C(Cl)C(Cl)=C(Cl)C([N+]([O-])=O)=C1Cl YXODCXKIYJZGJP-UHFFFAOYSA-N 0.000 description 3
- BPMOJGOPWSCNHJ-UHFFFAOYSA-N 1,3,5-trichloro-2,4-dinitrobenzene Chemical compound [O-][N+](=O)C1=C(Cl)C=C(Cl)C([N+]([O-])=O)=C1Cl BPMOJGOPWSCNHJ-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
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- 238000004448 titration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKEAMBAZBICIFP-UHFFFAOYSA-N 3-oxido-2,1,3-benzoxadiazol-3-ium Chemical compound C1=CC=CC2=[N+]([O-])ON=C21 OKEAMBAZBICIFP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FNYLWPVRPXGIIP-UHFFFAOYSA-N Triamterene Chemical compound NC1=NC2=NC(N)=NC(N)=C2N=C1C1=CC=CC=C1 FNYLWPVRPXGIIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- JDFUJAMTCCQARF-UHFFFAOYSA-N tatb Chemical compound NC1=C([N+]([O-])=O)C(N)=C([N+]([O-])=O)C(N)=C1[N+]([O-])=O JDFUJAMTCCQARF-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a method for measuring the content of homotrichlorotrinitrobenzene by a gas chromatography, belongs to the technical field of instrument analysis, and solves the problem of high measurement result deficiency in the prior art. The method provided by the invention uses SE-54 capillary column as chromatographic column, the temperature of the chromatographic column is 250-280 ℃, the temperature of the sample inlet is 260-280 ℃, the temperature of the FID detector is 290-310 ℃; adding chloroform into a trinitrobenzene sample to prepare a sample solution of 15-35 mg/ml; accurately sucking 1-5 mu L, rapidly injecting into gas chromatograph, and calculating content by area normalization method. By adopting the method, impurities and detected components can be completely separated, TCDNB content can be accurately measured, meanwhile, the content of TCTNB and T 4 CDNB can be detected, and the production condition of the product can be conveniently known; the occurrence of the phenomenon of the deficiency and high measurement result is avoided, and the accuracy of the analysis result is higher.
Description
Technical Field
The invention belongs to the technical field of instrument analysis, and particularly relates to a method for measuring the content of homotrichlorotrinitrobenzene by a gas chromatography method.
Background
And 3, 1,3, 5-trichloro-2, 4, 6-trinitrobenzene, which is also called TCTNB for short. Molecular formula C 6Cl3N3O6, molecular weight 316.5, white or pale yellow loose granular crystal, melting point 190-193 deg.C, density 1.93g/cm 3. Is not volatilized at normal temperature and pressure and does not absorb moisture. Heating to above 120 ℃ causes a slight sublimation phenomenon. Is soluble in benzene, toluene, xylene, acetone, dichloroethane and other organic solvents, and is insoluble in water.
TCTNB is an important explosive synthesis intermediate, is mainly used for synthesizing low-vulnerability explosive TATB, and can also be used for synthesizing trinitrobenzene triazide, benzofuroxan, trinitrotrimethylaminobenzene and other explosives. TCTNB is also a valuable explosive per se, with 0% impact sensitivity and 4% friction sensitivity, and can also be directly used as insecticide and bactericide. Can be obtained by nitration synthesis of trichlorphene (TCB for short) in fuming sulfuric acid and fuming nitric acid mixed acid, and the main synthesis principle is as follows:
The above reaction has two main by-products: 1,3, 5-trichloro-2, 6-dinitrobenzene (TCDNB for short) and 1,3,4, 5-tetrachloro-2, 6-dinitrobenzene (T 4 CDNB for short).
In the prior art, the quantitative measurement method of the homo-trichlorotrinitrobenzene comprises the following steps: and (3) hydrolyzing the homotrichlorotrinitrobenzene sample in an excessive alkaline solution, and titrating excessive alkali with hydrochloric acid standard after the reaction is completed, so as to determine the content of the homotrichlorotrinitrobenzene in the sample. By adopting the method, the reaction time of the homotrichlorotrinitrobenzene and the excessive alkali solution is longer, the titration end point color is changed from blue black to green to yellow, and the color is not easy to judge in the operation process. In addition, the sample contains 1,3, 5-trichloro-2, 6-dinitrobenzene and 1,3,4, 5-tetrachloro-2, 6-dinitrobenzene in addition to the main component of the sample. The chemical titration method can take part in chemical reaction together with the main components, so that the measurement result is high.
Therefore, the method for determining the homotrichlorotrinitrobenzene is simple, convenient to operate and accurate in determination result, and is a problem to be solved urgently by those skilled in the art.
Disclosure of Invention
The invention aims to provide a method for measuring the content of homotrichlorotrinitrobenzene by a gas chromatography, which can effectively separate the homotrichlorotrinitrobenzene and 1,3, 5-trichloro-2, 6-dinitrobenzene and 1,3,4, 5-tetrachloro-2, 6-dinitrobenzene obtained in a synthesis process, and has accurate results and simple and convenient operation.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for measuring the content of homotrichlorotrinitrobenzene by using a gas chromatography, which uses a SE-54 capillary column as a chromatographic column, wherein the temperature of the chromatographic column is 250-280 ℃, the temperature of a sample inlet is 260-280 ℃, and the temperature of a FID detector is 290-310 ℃.
In some embodiments of the invention, the column temperature is 270 ℃.
In some embodiments of the present invention, the sample inlet temperature is 265 ℃.
In some embodiments of the invention, the detector temperature is 300 ℃.
In some embodiments of the invention, the column size is 30m 0.53mm 1.5 μm.
In some embodiments of the invention, the method comprises the steps of:
Preparation of test solution: taking a homotrichlorotrinitrobenzene sample, and adding chloroform to prepare a sample solution of 15-35 mg/ml;
Accurately sucking 1-5 mu L of the sample solution, rapidly injecting into a gas chromatograph, separating each component of the sample solution by a chromatographic column, and calculating the content by adopting an area normalization method.
In some embodiments of the invention, the concentration of the test solution is 25mg/ml.
In some embodiments of the present invention, 1 μl of the test solution is accurately aspirated and rapidly injected into the gas chromatograph.
The sample of the homo-trichlorotrinitrobenzene is a product obtained by a synthesis process of the homo-trichlorotrinitrobenzene.
In one embodiment of the present invention, the chromatographic conditions are: the FID detector has a detector temperature of 300 ℃, a chromatographic column temperature of 270 ℃, a sample inlet temperature of 265 ℃ and chromatographic column specifications of 30m multiplied by 0.53mm multiplied by 1.5 mu m. Air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
Compared with the prior art, the invention has the following beneficial effects:
The invention has scientific design, ingenious conception, simple method, simple and convenient operation and accurate result. By adopting the method, impurities and tested components can be completely separated, the content of 1,3, 5-trichloro-2, 4, 6-trinitrobenzene can be accurately measured, and simultaneously the contents of 1,3, 5-trichloro-2, 6-trinitrobenzene and 1,3,4, 5-tetrachloro-2, 6-trinitrobenzene can be detected, so that the production condition of products can be conveniently known. The occurrence of the phenomenon of the deficiency and high measurement result is avoided, and the accuracy of the analysis result is higher.
The method shortens the analysis time. The chemical determination method in the prior art has the advantages of long saponification time, more manual operation steps, long time consumption and 4 hours for one determination, and can not meet the requirement of the process on the timeliness of analysis results. The method does not need to carry out special treatment on the sample, greatly shortens the analysis time, and only needs 1 hour for measurement.
The invention adopts the gas chromatography area normalization method to measure TCTNB content, has better repeatability, higher precision, convenient and quick operation, favorable production control and the like, and has better economic and social benefits. Plays a role in promoting and promoting the production of TCTNB.
Drawings
FIG. 1 is a TCTNB sample solution chromatogram of the present invention.
FIG. 2 is a chromatogram using SE-30 columns.
FIG. 3 is a chromatogram using an OV-101 column.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention relates to a method for measuring the content of homotrichlorotrinitrobenzene by a gas chromatography, which uses a SE-54 capillary column as a chromatographic column, wherein the temperature of the chromatographic column is 250-280 ℃, the temperature of a sample inlet is 260-280 ℃, and the temperature of a FID detector is 290-310 ℃.
Preferably, the column temperature is 270 ℃.
Preferably, the sample inlet temperature is 265 ℃.
Preferably, the detector temperature is 300 ℃.
Preferably, the column size is 30m by 0.53mm by 1.5 μm.
Preferably, the gas chromatography method according to the invention comprises the following steps:
Preparation of test solution: taking a homotrichlorotrinitrobenzene sample, and adding chloroform to prepare a sample solution of 15-35 mg/ml;
Accurately sucking 1-5 mu L of the sample solution, rapidly injecting into a gas chromatograph, separating each component of the sample solution by a chromatographic column, and calculating the content by adopting an area normalization method.
Preferably, the concentration of the test solution is 25mg/ml.
Preferably, 1. Mu.L of the sample solution is accurately aspirated and rapidly injected into the gas chromatograph.
The sample of the homo-trichlorotrinitrobenzene is a product obtained by a synthesis process of the homo-trichlorotrinitrobenzene.
The gas chromatograph used in the embodiment of the invention is an Agilent 7820A gas chromatograph.
Example 1
The solvent and the amount of the sample solution were examined in this example.
By looking at the data TCTNB is soluble in most organic solvents such as benzene, toluene, xylene, acetone, dichloroethane, etc., and insoluble in water. Benzene, toluene and xylene have high toxicity and high acetone volatility, so that ethanol, methanol, chloroform and the like are selected as solvents in the test.
0.5G of the homotrichlorotrinitrobenzene sample is taken, 30ml of ethanol, methanol and chloroform are respectively added, and the mixture is stirred. As a result, it was found that the absolute ethanol did not completely dissolve the sample; methanol also does not dissolve the sample completely. The chloroform can dissolve the whole sample. Therefore, chloroform is used as solvent.
0.5G of the homotrichlorotrinitrobenzene sample was taken and dissolved in 5ml, 10ml and 15ml of chloroform, respectively. As a result, it was found that when 10ml of chloroform was used for dissolution, some of the samples were not completely dissolved. When the amount of chloroform was 15ml, the sample was completely dissolved. In order to ensure complete dissolution of the sample, the amount of chloroform was determined to be 20ml taking into account the amount of solvent.
Example 2
The effect of measuring the homotrichlorotrinitrobenzene sample by adopting SE-30, OV-101 and SE-54 chromatographic columns is examined in the embodiment, and the method specifically comprises the following steps:
taking 0.5g of a homotrichlorotrinitrobenzene sample, adding 20ml of chloroform for dissolution, filtering, taking 1 mu L of continuous liquid, and rapidly injecting into a gas chromatograph.
The chromatographic conditions are as follows: the FID detector has a detector temperature of 300 ℃, a chromatographic column temperature of 270 ℃, a sample inlet temperature of 265 ℃ and chromatographic column specifications of 30m multiplied by 0.53mm multiplied by 1.5 mu m. Air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
When SE-54 chromatographic column is used, each component can be effectively separated, and the solvent peak is not interfered, as shown in figure 1. In FIG. 1, peak 1 is the solvent peak, peak 2 is TCDNB, peak 3 is TCTNB, and peak 4 is T 4 CDNB. Therefore, in the method of the invention, the peak area normalization method can be used for calculating the content of each component.
TCTNB and T 4 DNB were not efficiently separated when measured using SE-30 columns as shown in FIG. 2. Peak 1 in fig. 2 is the solvent peak, peak 2 is TCDNB, and peak 3 is the mixed peak of TCTNB and T 4 CDNB.
TCTNB and T 4 DNB were not efficiently separated when measured using OV-101 columns, as shown in FIG. 3. Peak 1 in fig. 2 is the solvent peak, peak 2 is TCDNB, and peak 3 is the mixed peak of TCTNB and T 4 CDNB.
Example 3
The temperature of the chromatographic column is examined in the embodiment, and the specific steps are as follows:
taking 0.5g of a homotrichlorotrinitrobenzene sample, adding 20ml of chloroform for dissolution, filtering, taking 1 mu L of continuous liquid, and rapidly injecting into a gas chromatograph.
The chromatographic conditions are as follows: FID detector with detector temperature of 300 deg.C, SE-54 chromatographic column with specification of 30mX0.53 mm×1.5 μm; the sample inlet temperature was 265 ℃. Air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
As a result, it was found that the peak shape of each of the chromatographic peaks was relatively broad and TCTNB overlapped with the chromatographic peak of T 4 DNB at the column temperature of 220 ℃. The separation effect is improved when the temperature is raised to 250 ℃, but the peak shape is wider and the peak tip is positioned behind. After the temperature is increased to 270 ℃, the components can be completely separated, and the peak shape is symmetrical and narrow.
Example 4
The sample concentration was examined in this example: taking 0.5g of a homotrichlorotrinitrobenzene sample, adding chloroform for dissolution, preparing test solution with the concentration of 15mg/mL, 25mg/mL and 35mg/mL, filtering, taking 1 mu L of continuous liquid, and rapidly injecting into a gas chromatograph.
The chromatographic conditions are as follows: FID detector with detector temperature of 300 deg.C, SE-54 chromatographic column with specification of 30mX0.53 mm×1.5 μm; the sample inlet temperature was 265 ℃. Air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
As a result, it was found that each component was efficiently separated in the chromatograms obtained for the three concentrations of the test sample solutions.
Example 5
In the embodiment, the temperature of the sample inlet is examined, the temperature of the sample inlet is respectively set to 260 ℃, 270 ℃ and 280 ℃, and the separation condition of each component under the condition of different sample inlet temperatures is examined. The method comprises the following steps:
taking 0.5g of a homotrichlorotrinitrobenzene sample, adding 20ml of chloroform for dissolution, filtering, taking 1 mu L of continuous liquid, and rapidly injecting into a gas chromatograph.
The chromatographic conditions are as follows: FID detector with detector temperature of 300 deg.C, SE-54 chromatographic column with specification of 30mX0.53 mm×1.5 μm; air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
As a result, it was found that each component was effectively separated at a sample inlet temperature of 260℃and 270℃and 280 ℃.
Example 6
This example examined the reproducibility of the method of the invention. The same sample was selected and, under normal and correct operating conditions, 20 single tests were performed on the sample by the same operator, in the same laboratory, using the same instrument, and in a short period of time.
The sample concentration is: 25mg/mL, the sample injection amount was 1. Mu.L.
The chromatographic conditions are as follows: FID detector with detector temperature of 300 deg.C, SE-54 chromatographic column with specification of 30mX0.53 mm×1.5 μm; the sample inlet temperature was 280 ℃. Air: 300mL/min, flow: 1.5mL/min, H 2: 30mL/min, split ratio: 5:1.
The test results are shown in the following table.
TABLE 1 repeatability test results
As can be seen from Table 1, TCDNB had a range of 0.14% and a standard deviation of 0.04%; TCTNB has a range of 0.11% and a standard deviation of 0.04%; the range of T4CDNB was 0.14% and the standard deviation was 0.05%. The extremely bad results are not more than 0.20% of the test requirements, and the obtained results have higher precision.
The method is proved to have good reproducibility.
The above embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or color changes made in the main design concept and spirit of the present invention are still consistent with the present invention, and all the technical problems to be solved are included in the scope of the present invention.
Claims (7)
1. The method for measuring the content of the homo-trichlorotrinitrobenzene by using the gas chromatography is characterized in that a SE-54 capillary column is used as a chromatographic column, the temperature of the chromatographic column is 250-280 ℃, the temperature of a sample inlet is 260-280 ℃, and the temperature of a FID detector is 290-310 ℃;
The method comprises the following steps:
Preparation of test solution: taking a homotrichlorotrinitrobenzene sample, and adding chloroform to prepare a sample solution of 15-35 mg/ml;
Accurately sucking 1-5 mu L of the sample solution, rapidly injecting into a gas chromatograph, separating each component of the sample solution by a chromatographic column, and calculating the content by adopting an area normalization method;
the homo-trichlorotrinitrobenzene sample is a product obtained by a synthesis process of the homo-trichlorotrinitrobenzene.
2. The method for determining the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein the temperature of a chromatographic column is 270 ℃.
3. The method for determining the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein the temperature of a sample inlet is 265 ℃.
4. The method for determining the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein the temperature of the detector is 300 ℃.
5. The method for determining the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein the specification of the chromatographic column is 30m multiplied by 0.53mm multiplied by 1.5 μm.
6. The method for determining the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein the concentration of the test solution is 25mg/ml.
7. The method for measuring the content of the homotrichlorotrinitrobenzene by using the gas chromatography according to claim 1, wherein 1 μl of the test solution is accurately sucked and rapidly injected into the gas chromatograph.
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Citations (3)
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| CN104502477A (en) * | 2014-12-23 | 2015-04-08 | 南宁化工股份有限公司 | Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid |
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